US8312739B2 - Dual stage ion exchange for chemical strengthening of glass - Google Patents

Dual stage ion exchange for chemical strengthening of glass Download PDF

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US8312739B2
US8312739B2 US12/510,599 US51059909A US8312739B2 US 8312739 B2 US8312739 B2 US 8312739B2 US 51059909 A US51059909 A US 51059909A US 8312739 B2 US8312739 B2 US 8312739B2
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glass
metal
ions
bath
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US20100028607A1 (en
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Christopher Morton Lee
Lawrence George Mann
Jose Mario Quintal
Yongsheng Yan
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Corning Inc
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Corning Inc
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/005—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to introduce in the glass such metals or metallic ions as Ag, Cu
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness

Definitions

  • the invention relates to chemical strengthening of glasses. More particularly, the invention relates to the use of ion exchange processes to strengthen glasses. Even more particularly, the invention relates to a process comprising multiple ion exchange processes.
  • Chemically strengthened glass have recently been identified for use in hand held devices, such as mobile phones, media players, and other devices, as well as other applications requiring transparency, high strength and abrasion resistance.
  • Ion exchange is a chemical strengthening process that starts with a glass containing smaller ions (effluent ions) that are capable of exchange with larger ions (exchange ions) in a molten salt bath at elevated temperatures—i.e., the larger ions replace the smaller ions in the glass.
  • the larger, densely packed ions at the glass surface generate a high compressive stress, which in turn provides higher strength.
  • the salt bath becomes increasingly diluted by the smaller effluent ions (counter ions) that are exchanged out of the glass.
  • Salt counter ion concentration increases proportionally with the volume or number of glass parts that are ion exchanged in a salt bath. Whereas “fresh” unused salt provides the highest compressive strength, every subsequent ion exchange run increases the concentration of the smaller ions that are exchanged out of the glass and into the molten salt bath. Conversely, the concentration of the salt that provides the larger ions in the bath decreases. With continued use of the same bath, the compressive stress of the finished products is reduced.
  • the increased dilution of the bath is typically compensated for by replacing at least a portion of the salt bath, based on ion exchange production volume or when the compressive stress of the ion exchanged glass reaches a minimum acceptable value. While such practices are adequate to maintain a minimal compressive stress in the glass, they result in significant variability and constant cyclical fluctuation in compressive stress of chemically strengthened glasses during production.
  • DIOX dual stage ion exchange
  • the glass undergoes ion exchange in a first, “fresh” salt bath followed by a second ion exchange in a second salt bath that has a diluted effluent ion concentration.
  • This method sacrifices the compressive stress of the surface of the glass. This is unacceptable in hand held device applications, because it does not provide protection from surface flaws that are introduced by contact forces that may be encountered during common use of the device.
  • the present invention provides a method of chemically strengthening a glass.
  • the method includes ion exchange of the glass in a first bath, followed by immersion in the second bath.
  • the first bath is diluted with an effluent ion, and the second bath having a smaller concentration of the effluent ion than the first bath.
  • the method provides a compressive stress at the surface that is sufficient to arrest flaws introduced by contact forces at the surface of the glass while having sufficiently deep compressive depth-of-layer for high reliability.
  • one aspect of the invention is to provide a method of strengthening a glass.
  • the method comprises creating a compressive stress in an outer region of the glass extending from a surface of the glass to a depth-of-layer, the compressive stress being sufficient to arrest flaws within the glass and to arrest flaws at the surface introduced by contact forces at the surface.
  • the compressive stress is created by: providing a glass having a plurality of first metal ions within the outer region; ion exchanging a first portion of the plurality of first metal ions in the outer region of the glass with a plurality of second metal ions in a first salt bath, wherein the first salt bath is diluted with a first concentration of the first metal ions; and ion exchanging a second portion of the plurality of the first metal ions in the outer region of the glass with a plurality of the second metal ions in a second salt bath, wherein the second salt bath has a second concentration of the first metal that is less than the first concentration.
  • a second aspect of the invention is to provide a method of strengthening a glass.
  • the method comprising the steps of: providing a glass, the glass comprising a plurality of ions of a first metal, each of the ions having a first ionic radius; immersing the glass in a first ion exchange bath, the first ion exchange bath comprising a plurality of ions of a second metal and a first concentration of ions of the first metal, wherein each of the ions of the second metal has a second ionic radius, the second ionic radius being greater than the first ionic radius; and immersing the glass in a second ion exchange bath after immersing the glass in the first ion exchange bath, the second ion exchange bath comprising a plurality of ions of the second metal and a second concentration of ions of the first metal, wherein the second concentration is less than the first concentration, wherein a portion of the plurality of ions of the first metal in the glass are replaced by ions of the second metal to create
  • a third aspect of the invention is to provide a method of reducing variability of compressive stress in a chemically strengthened glass article.
  • the method comprises the steps of: providing a glass article, the glass comprising a plurality of ions of a first metal, each of the ions having a first ionic radius; immersing the glass article in a first ion exchange bath, the first ion exchange bath comprising a plurality of ions of a second metal and a first concentration of ions of the first metal, wherein each of the ions of the second metal has a second ionic radius, the second ionic radius being greater than the first ionic radius; and immersing the glass article in a second ion exchange bath after immersing the glass in the first ion exchange bath, the second ion exchange bath comprising a plurality of ions of the second metal and a second concentration of ions of the first metal, wherein the second concentration is less than the first concentration.
  • FIG. 1 is a plot of compressive stress versus dilution with NaNO 3 of primary and secondary ion exchange salt baths
  • FIG. 2 is a plot of destructive four point bend surface stress measurements versus dilution with NaNO 3 of primary and secondary salt baths
  • FIG. 3 is a plot of ring on ring force loading results versus dilution with NaNO 3 of primary and secondary salt baths
  • FIG. 4 is a plot of ring on ring force loading results versus dilution with NaNO 3 of primary and secondary salt baths for abraded glass samples.
  • FIG. 5 is a plot of ball drop height results versus dilution with NaNO 3 of primary and secondary salt baths.
  • CS Surface compressive stress
  • DOL depth of layer
  • Factors that can reduce achievable CS include salt counter ion concentration (the concentration of the effluent ion in the molten salt bath), higher processing temperatures, and long processing times that are needed to obtain adequate DOL. Whereas processing time and temperature can be controlled, salt counter ion concentration increases proportionally to the volume or number of glass parts that are ion exchanged in the salt bath. “Fresh” salt (i.e., salt newly introduced to the bath) provides the highest CS in chemically strengthened glass. Every subsequent run, however, increases the concentration of the small ions exchanged out of the glass into the molten salt bath.
  • the concentration of the salt that provides the larger ions decreases with each glass part strengthened in a bath, consequently reducing CS of finished product, despite carrying out the ion exchange process at constant temperature and time. In high volume production, significant variability in compressive strength may therefore be observed from one glass article to the next.
  • a dual stage ion exchange (DIOX) process for strengthening glass and reducing the variability of compressive stress in glass is provided and described herein.
  • the process is capable of maintaining a high, and stable, surface compressive strength when chemically strengthening a number of glass articles in a production setting.
  • the process includes a first or primary exchange and a second (secondary) exchange.
  • the glass is strengthened to a desired depth of layer (DOL) in a first molten salt bath.
  • the first molted salt bath that is diluted with effluent, or exchangeable (i.e., effluent ions, or ions that are exchanged out of the glass and replaced by larger ions), metal ions (also referred to herein as “ions”).
  • the salt bath is diluted with Na + ions.
  • the presence of the effluent ions in the bath decreases the compressive stress of the glass parts.
  • each additional ion exchange run does not significantly change the percentage of effluent ions in the bath, and the compressive stress therefore does not degrade as rapidly as would be the case for an undiluted salt bath.
  • the glass strengthened in the primary exchange is then chemically strengthened in a second stage molten salt bath that containing the same exchange ions, with much lower (or zero) effluent ion concentration than in the first stage bath, to restore the compressive stress to the desired level.
  • a second stage molten salt bath that containing the same exchange ions, with much lower (or zero) effluent ion concentration than in the first stage bath, to restore the compressive stress to the desired level.
  • the rate or degree of salt dilution is significantly reduced in the second stage.
  • the dual stage ion exchange process described herein is capable of maintaining consistently high compressive stress in the final glass product, despite increasing effluent ion dilution rate in the primary stage bath.
  • This process is also expected to have more efficient salt utilization by allowing the primary salt bath to be used to a point where the compressive stress after the primary ion exchange is below a lower CS specification limit.
  • the process also minimizes equipment downtime associated with salt replacement and provides improved process stability, higher compressive strength values, more efficient salt utilization, and overall higher mechanical reliability of products.
  • the glass is an alkali aluminosilicate glass.
  • the alkali aluminosilicate glass comprises, consists essentially of, or consists of: 60-70 mol % SiO 2 ; 6-14 mol % Al 2 O 3 ; 0-15 mol % B 2 O 3 ; 0-15 mol % Li 2 O; 0-20 mol % Na 2 O; 0-10 mol % K 2 O; 0-8 mol % MgO; 0-10 mol % CaO; 0-5 mol % ZrO 2 ; 0-1 mol % SnO 2 ; 0-1 mol % CeO 2 ; less than 50 ppm As 2 O 3 ; and less than 50 ppm Sb 2 O 3 ; wherein 12 mol % ⁇ Li 2 O+Na 2 O+K 2 O ⁇ 20 mol % and 0 mol % ⁇ MgO+CaO ⁇ 10 mol %.
  • the alkali aluminosilicate glass comprises, consists essentially of, or consists of: 64 mol % ⁇ SiO 2 ⁇ 68 mol %; 12 mol % ⁇ Na 2 O ⁇ 16 mol %; 8 mol % ⁇ Al 2 O 3 ⁇ 12 mol %; 0 mol % ⁇ B 2 O 3 ⁇ 3 mol %; 2 mol % ⁇ K 2 O ⁇ 5 mol %; 4 mol % ⁇ MgO ⁇ 6 mol %; and 0 mol % ⁇ CaO ⁇ 5 mol %, and wherein: 66 mol % ⁇ SiO 2 +B 2 O 3 +CaO ⁇ 69 mol %; Na 2 O+K 2 O+B 2 O 3 +MgO+CaO+SrO>10 mol %; 5 mol % ⁇ MgO+CaO+SrO ⁇ 8 mol %; (Na 2 O+B 2 O 3 ) ⁇ Al 2 O
  • the alkali aluminosilicate glass is, in some embodiments, substantially free of lithium, whereas in other embodiments, the alkali aluminosilicate glass is substantially free of at least one of arsenic, antimony, and barium. In other embodiments, the alkali aluminosilicate glass is down-drawable by those techniques known in the art, such as, but not limited to, fusion-draw processes, slot-draw processes, and re-draw processes.
  • the alkali aluminosilicate glass has the composition: 66.7 mol % SiO 2 ; 10.5 mol % Al 2 O 3 ; 0.64 mol % B 2 O 3 ; 13.8 mol % Na 2 O; 2.06 mol % K 2 O; 5.50 mol % MgO; 0.46 mol % CaO; 0.01 mol % ZrO 2 ; 0.34 mol % As 2 O 3 ; and 0.007 mol % Fe 2 O 3 .
  • the alkali aluminosilicate glass has the composition: 66.4 mol % SiO 2 ; 10.3 mol % Al 2 O 3 ; 0.60 mol % B 2 O 3 ; 4.0 mol % Na 2 O; 2.10 mol % K 2 O; 5.76 mol % MgO; 0.58 mol % CaO; 0.01 mol % ZrO 2 ; 0.21 mol % SnO 2 ; and 0.007 mol % Fe 2 O 3 .
  • the primary and secondary salt baths are prepared by adding the desired amount of effluent salt and the salt of the ion to be exchanged with the effluent in the glass.
  • the ions are alkali metal ions—i.e., Li + , Na + , K + , Cs + , and Rb + . Larger alkali metal ions in the bath replace smaller alkali metal ions in the glass.
  • Li + ions in the glass may be replaced with Na + , K + , Cs + , or Rb + ions
  • Na + ions in the glass may be replaced with K + , Cs + , or Rb + ions, and so on.
  • the alkali metal ions in the glass are exchanged with ions of the next largest alkali metal ion.
  • Na + ions in the glass is usually exchanged with K + ions in the bath.
  • the salt (or salts) is melted and heated to a predetermined temperature, typically in a range from about 380° C. up to about 450° C., and the bath is held at that temperature to stabilize for a predetermined time. In one embodiment, the salt bath is held at temperature for about 12 hours. It will be appreciated by those skilled in the art that other temperatures and stabilization times may be used.
  • “fresh” unused salt may be used to prepare the primary stage bath.
  • a previously diluted salt bath may be used as the primary salt bath. It is preferred that fresh salt be used to prepare the secondary bath salt bath, although a previously used bath having a considerably lower salt dilution than the primary stage bath may be used instead.
  • glass samples Prior to immersion in the primary salt bath, glass samples are pre-heated to prevent thermal shock and minimize bath loading (i.e., cooling) effects.
  • the pre-heating temperature depends on the temperature of the salt bath.
  • the sample is then immersed in the primary bath, and the primary ion exchange stage is carried out at a first predetermined temperature for a time sufficient to achieve a desired depth of layer, at which point the glass sample is removed from the primary salt bath and allowed to cool.
  • the glass sample may be rinsed with water to remove residual dried salt and to prevent contamination of the secondary stage bath, and then dried to remove residual moisture.
  • the glass may optionally be annealed between respective immersions in the primary and secondary salt baths.
  • the glass sample Before immersion in the secondary ion exchange bath, the glass sample is again pre-heated.
  • the secondary ion exchange stage is carried out in the secondary stage bath having either fresh salt (or a significantly lower dilution rate than the primary stage) to increase or stabilize the compressive stress created in the primary stage ion exchange.
  • the sample is immersed in the bath, and the secondary ion exchange stage is carried out at a second predetermined temperature for a time sufficient to achieve the desired compressive stress, at which point the glass sample is removed from the secondary salt bath and allowed to cool.
  • the glass sample may be rinsed with water to remove residual dried salt and to prevent contamination of the secondary stage bath, and then dried to remove residual moisture.
  • Compressive stress resulting from the chemical strengthening process described herein can be measured using either non-destructive methods, such as, for example, the Orihara FSM-6000 stress-optical meter, which measures surface compressive stress, or destructive tests such as four point bend, three point bend, ring on ring, ball drop tests, and the like.
  • non-destructive methods such as, for example, the Orihara FSM-6000 stress-optical meter, which measures surface compressive stress, or destructive tests such as four point bend, three point bend, ring on ring, ball drop tests, and the like.
  • a KNO 3 salt bath was purposely diluted with 0 wt %, 2.5 wt %, 5 wt %, 7.5 wt %, and 10 wt % NaNO 3 to simulate deteriorating salt bath composition under high volume production conditions.
  • Groups of alkali aluminosilicate glass samples were ion exchanged at 412° C. at each dilution level for 270 minutes.
  • a subset from each group of samples was then ion exchanged in a bath containing fresh KNO 3 salt and a residual amount of NaNO 3 salt at approximately 410° C., for 120 minutes.
  • FIG. 1 is a plot of compressive stress versus dilution with NaNO 3 of the primary (IOX) and secondary (DIOX) ion exchange salt baths.
  • the compressive stress of the samples after the primary or single stage of the ion exchange process steadily declines from 710 MPa to 477 MPa, as the NaNO 3 dilution increases from approximately 0 to 10 wt %.
  • the average compressive stress recovers back to 750 to 765 MPa, which is comparable to the compressive stress observed for samples that have undergone single ion exchange with a fresh KNO 3 bath.
  • FIG. 2 is a plot of destructive four point bend surface stress measurements versus dilution with NaNO 3 of the primary (IOX) and secondary (DIOX) salt baths.
  • the compressive stress of the samples after the primary or single stage of the ion exchange process steadily declines from 700 MPa to 520 MPa, as the NaNO 3 dilution increases from approximately 0 to 10 wt %.
  • the average compressive stress recovers to 700 to 790 MPa, which is comparable to single ion exchange with a fresh KNO 3 bath.
  • the results shown in FIG. 2 correlate with the compressive stress results shown in FIG. 1 .
  • Weibull plots show that the parts subjected to the fresh bath second stage ion exchange have significantly higher four point bend strength than those subjected to only single stage ion exchange having steadily increasing NaNO 3 dilution levels that are typical in high volume manufacturing.
  • FIG. 3 is a plot of ring on ring force loading results versus dilution with NaNO 3 of the primary (IOX) and secondary (DIOX) salt baths.
  • the force loading steadily declines from 1800 N to 1320 N after single stage ion exchange, as the NaNO 3 dilution increases from approximately 0 to 10 wt %. After these parts are ion exchanged in a second fresh bath, the average force loading recovers to 1900 to 2000 N, which is comparable to single ion exchange with a fresh KNO 3 bath.
  • the results shown in FIG. 3 correlate with the compressive stress results shown in FIG. 1 .
  • FIG. 4 is a plot of ring on ring force loading results versus dilution with NaNO 3 of the primary (IOX) and secondary (DIOX) salt baths for glass samples that had been abraded or “aged” as described hereinabove.
  • Force loading steadily declines from 1320 N to 770 N after single stage ion exchange, as the NaNO 3 dilution increases from approximately 0 to 10 wt %. After these parts are ion exchanged in a second fresh bath, the average force loading of abraded samples recovers to 1400 to 1700 N.
  • the results shown in FIG. 3 correlate with the compressive stress results shown in FIG. 1 .
  • FIG. 3 When compared with ring on ring results obtained for “virgin” (unabraded) samples ( FIG.
  • FIG. 5 is a plot of ball drop height results versus dilution with NaNO 3 of the primary (IOX) and secondary (DIOX) salt baths.
  • the average ball drop height steadily decline from 165 cm to 115 cm after single stage ion exchange, as the NaNO 3 dilution increases from approximately 0 to 10 wt %. After these parts are ion exchanged in a second fresh bath, the average ball drop height recovers back to 155 cm to 185 cm, which is comparable to single ion exchange with a fresh KNO 3 bath.
  • the results shown in FIG. 5 correlate with the compressive stress results shown in FIG. 1 .
  • Weibull plots show that the parts subjected to the fresh bath second stage ion exchange have significantly higher ball drop heights than those subjected to only single stage ion exchange having steadily increasing NaNO 3 dilution levels that are typical in high volume manufacturing.

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  • Engineering & Computer Science (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • Surface Treatment Of Glass (AREA)
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CN102137822B (zh) 2015-12-09
CN102137822A (zh) 2011-07-27
JP2011529438A (ja) 2011-12-08
US20100028607A1 (en) 2010-02-04
EP2321230A4 (en) 2012-10-10
WO2010014163A1 (en) 2010-02-04
JP5777109B2 (ja) 2015-09-09
EP2321230A1 (en) 2011-05-18
KR20110038701A (ko) 2011-04-14

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